EP1369043B1 - Use of beads as food additives - Google Patents

Use of beads as food additives Download PDF

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Publication number
EP1369043B1
EP1369043B1 EP03018435A EP03018435A EP1369043B1 EP 1369043 B1 EP1369043 B1 EP 1369043B1 EP 03018435 A EP03018435 A EP 03018435A EP 03018435 A EP03018435 A EP 03018435A EP 1369043 B1 EP1369043 B1 EP 1369043B1
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EP
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Prior art keywords
flavour
beads
water
alginate
use according
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EP03018435A
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German (de)
English (en)
French (fr)
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EP1369043A1 (en
Inventor
Johnny Bouwmeesters
Kris De Roos
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Givaudan SA
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Givaudan SA
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L13/00—Meat products; Meat meal; Preparation or treatment thereof
    • A23L13/50—Poultry products, e.g. poultry sausages
    • A23L13/55—Treatment of original pieces or parts
    • A23L13/57—Coating with a layer or stuffing
    • A—HUMAN NECESSITIES
    • A21—BAKING; EDIBLE DOUGHS
    • A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
    • A21D13/00—Finished or partly finished bakery products
    • A21D13/20—Partially or completely coated products
    • A21D13/22—Partially or completely coated products coated before baking
    • A—HUMAN NECESSITIES
    • A21—BAKING; EDIBLE DOUGHS
    • A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
    • A21D13/00—Finished or partly finished bakery products
    • A21D13/20—Partially or completely coated products
    • A21D13/28—Partially or completely coated products characterised by the coating composition
    • A—HUMAN NECESSITIES
    • A21—BAKING; EDIBLE DOUGHS
    • A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
    • A21D2/00—Treatment of flour or dough by adding materials thereto before or during baking
    • A21D2/08—Treatment of flour or dough by adding materials thereto before or during baking by adding organic substances
    • A21D2/14—Organic oxygen compounds
    • A21D2/18—Carbohydrates
    • A21D2/183—Natural gums
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/04—Production of frozen sweets, e.g. ice-cream
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
    • A23G9/42—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds containing plants or parts thereof, e.g. fruits, seeds, extracts
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/44—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by shape, structure or physical form
    • A23G9/48—Composite products, e.g. layered, laminated, coated, filled
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/52—Liquid products; Solid products in the form of powders, flakes or granules for making liquid products ; Finished or semi-finished solid products, frozen granules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L13/00—Meat products; Meat meal; Preparation or treatment thereof
    • A23L13/40—Meat products; Meat meal; Preparation or treatment thereof containing additives
    • A23L13/42—Additives other than enzymes or microorganisms in meat products or meat meals
    • A23L13/428—Addition of flavours, spices, colours, amino acids or their salts, peptides, vitamins, yeast extract or autolysate, nucleic acid or derivatives, organic acidifying agents or their salts or acidogens, sweeteners, e.g. sugars or sugar alcohols; Addition of alcohol-containing products
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
    • A23L27/72—Encapsulation
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A23L29/272—Gellan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L7/00—Cereal-derived products; Malt products; Preparation or treatment thereof
    • A23L7/10—Cereal-derived products
    • A23L7/109—Types of pasta, e.g. macaroni or noodles
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L7/00—Cereal-derived products; Malt products; Preparation or treatment thereof
    • A23L7/10—Cereal-derived products
    • A23L7/161—Puffed cereals, e.g. popcorn or puffed rice
    • A23L7/165—Preparation of puffed cereals involving preparation of meal or dough as an intermediate step
    • A23L7/17—Preparation of puffed cereals involving preparation of meal or dough as an intermediate step by extrusion
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10—Coating with edible coatings, e.g. with oils or fats
    • A23P20/12—Apparatus or processes for applying powders or particles to foodstuffs, e.g. for breading; Such apparatus combined with means for pre-moistening or battering
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G2200/00—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents
    • A23G2200/14—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents containing fruits, nuts, e.g. almonds, seeds, plants, plant extracts or essential oils
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • the present invention relates to the use of beads as food additives in harsh food processes.
  • flavour systems A frequent problem associated with the application of flavour systems is the loss of flavour by volatilization or chemical decomposition.
  • the harsh environment of some food processes such as baking, extruding, retorting and deep frying, to name a few, creates unique problems for the survival of flavours in finished food products.
  • the loss of flavour usually results in flavour profile distortion or even in complete loss of flavour. Therefore, food scientists and application specialists are continuously searching for methods to protect flavours against volatilization and decomposition during processing.
  • the first category of encapsulated flavours consists of water-soluble particles containing a dispersion of flavour oil.
  • a number of water-soluble carrier materials are employed in the production of this type of encapsulated flavours, such as sugars, modified starches and gums.
  • the industry commonly utilizes spray drying, extrusion and fluidized bed coating to produce the particles.
  • Flavours encapsulated in a water-soluble matrix can be used for controlling flavour delivery and improving flavour stability in dry products such as chewing gum, pressed tablets and dry mixes for the preparation of instant soups, beverages, sauces and desserts.
  • this type of encapsulation is unsuitable for improving flavour performance in products that contain water because of dissolution of particulate flavouring materials. Since in the preparation of most foods, water is involved at any stage of the processing, encapsulation in water-soluble matrices has limited applicability for improving flavour stability or for controlling flavour retention and release.
  • fat encapsulation is sometimes being used (second category).
  • second category the use of fat-encapsulated flavours is limited to food products that are processed at relatively low temperatures, because at temperatures above the melting point of the fat much of the effectiveness of the encapsulation is lost. In practice, this means that fat encapsulation can not effectively be used for controlled flavour delivery in products that are heated above 80°C which comprises the majority of products that is boiled, baked, roasted, (deep) fried or extruded.
  • the third category of encapsulated flavours consists of particles that are water- insoluble and heat-stable.
  • the methods currently being used to prepare such particles are micro-encapsulation by coacervation and encapsulation in microorganisms.
  • micro-encapsulation by coacervation creates a barrier of protein around a droplet of flavour oil.
  • This barrier provides improved flavour retention during heat processing and higher shelf-life stability.
  • it can provide improved flavour performance through enhanced flavour release during consumption as, for example, in chewing gum.
  • the coacervation microparticles release the flavour by fracturing the protein membrane surrounding the flavour oil during mastication. For optimum results, it is important that the capsules are "engineered” for high flavour retention during processing without adversely affecting flavour release.
  • Both microbial cells and coacervation microcapsules are able to survive food processes such as baking, extruding, retorting and deep frying.
  • the major risk for this type of capsules is that they are ruptured during the process as a consequence of the shear forces applied during mixing, grinding or other high-shear processes to which the product is subjected during its production.
  • salts of anionic polysaccharides such as the calcium salts of alginic acid, pectin and gellan gum.
  • Calcium alginate in particular, has found useful application as a water insoluble matrix for the encapsulation of microbial cells ( T. Shiotani and T. Yamane, Eur. J. Appl. Microbiol. Biotechnol. 13 (2) 96-101 [1981] , H.C. Provost, Divies and T. Rousseau, Biotechnol. Lett. 7 (4) 247-52 [1985] ), enzymes ( P. Brodelius and K. Mosbach, Adv. Appl. Microbiol.
  • alginate for controlled flavour delivery is described in European patent application 0 221 850 .
  • This encapsulation in calcium alginate is used for controlled delivery of water-insoluble flavours from chewing gum.
  • the process for encapsulation involves separation of the alginate matrix from a large excess of water followed by air drying. Therefore, this process is not suitable for encapsulation of water-soluble and volatile flavours, because these compounds either remain in the aqueous phase or volatilize during drying.
  • the approach does not allow control of flavour release by variation of particle size, porosity and flavour solvent composition.
  • the demand is fulfilled by beads made by a particular method.
  • the invention therefore provides the use of polysaccharide-based beads prepared by a process as hereinunder described in foods that are subjected to harsh processing conditions such as baking, extruding, retorting and deep frying.
  • the beads consist of a matrix of a reticulated multivalent cation-containing acid polysaccharide and at least one water-soluble and/or volatile liquid active ingredient and/or one water soluble and/or volatile solid active ingredient filling at least partly the voids built by the acid polysaccharide.
  • the active ingredient is at least one compound of the group consisting of flavours, fragrances, vitamins or colouring materials.
  • the active ingredient is particularly a liquid or solid flavour, in particular a flavour oil, or a flavour dissolved in oil.
  • Said multivalent cation -containing acid polysaccharide is preferably an alginate, especially calcium alginate.
  • Said acid polysaccharide may be a pectin, especially a low ester pectin, preferably with a degree of esterification of less than 5% by weight.
  • the acid polysaccharide may also be gellan gum.
  • the beads are heat-stable and the active ingredient is released over time. Further, the beads are mechanically stable and have a diameter of about 10 to about 5000 ⁇ m, preferably of 100-1500 ⁇ m, specifically of 400-1200 ⁇ m.
  • the process comprises the steps of:
  • the active ingredient is at least one compound of the group consisting of flavours, fragrances, vitamins or colouring materials.
  • the invention further provides beads as hereinabove described and capable of withstanding harsh food processing conditions, prepared by a process as hereinabove described.
  • the water-immiscible material is a lipid, in particular a vegetable oil, a fat, a mono- or diglyceride, or a lipophilic fat replacer, especially a sucrose polyester.
  • Said acid polysaccharide in the form of an alkali metal salt is preferably as an alginate, especially sodium alginate.
  • Said acid polysaccharide may be a pectin, especially a low ester pectin, preferably one having a degree of esterification of less than 5% by weight.
  • the acid polysaccharide may also be gellan gum.
  • the emulsifier may be a modified starch, especially an octenyl succinated starch.
  • the water-soluble substance may be a polysaccharide, the polysaccharide preferably being at least one of the group consisting of maltodextrin, modified cellulose, especialy methyl or ethyl cellulose, locust bean gum, dextran, gum arabic and konjac.
  • a protein is preferred as the water-soluble substance.
  • the water-dispersible substance may be an adsorbent, especially silicon dioxide.
  • the multivalent ions may be ions selected from the group consisting of calcium, strontium, barium, iron, silver, aluminium, manganese, copper and zinc, especially calcium ions.
  • Said forming of discrete droplets may be generated by a spraying method known per se, especially by pouring the system on a rotating disk, or by extruding or pumping said system through an orifice or a needle at a rate slow enough to prevent the formation of a jet, or by building a jet of said system and breaking up said jet by means of a resonance technique known per se, e.g. vibration or pulsation.
  • a spraying method known per se especially by pouring the system on a rotating disk, or by extruding or pumping said system through an orifice or a needle at a rate slow enough to prevent the formation of a jet, or by building a jet of said system and breaking up said jet by means of a resonance technique known per se, e.g. vibration or pulsation.
  • the beads may be isolated from the suspension by filtration or centrifugation, thereby yielding moist beads, which beads may be dried, especially in an oven or fluid bed dryer.
  • the moist beads are dried in the presence of an anti-caking agent, especially in the presence of starch, maltodextrine or silicon dioxide.
  • Said loading of the moist or dry beads with at least one active ingredient is advantageously performed by contacting the active ingredient(s) with the moist beads at room or elevated temperature and allowing the active ingrdient(s) to be absorbed or adsorbed into the beads.
  • the beads according to the invention that are preferably prepared by the abovementioned process can be used in a method for flavouring, perfuming, vitaminizing or colouring food, which comprises adding the beads to the food in an effective amount, whereby the addition of the beads to the food can be performed prior to or during an extruding step of the food product or by coating the food with said beads or even prior to frying or baking the food because of their mechanical stability.
  • the present invention allows the encapsulation of water-soluble and/or volatile flavours, vitamins, colouring materials and other active ingredients into a water-insoluble, heat-stable polysaccharide matrix in such a way that the performance of the encapsulated ingredient in the application is improved by reducing the risk of flavour loss by volatilization or chemical decomposition during (heat) processing.
  • the method allows encapsulation of water-soluble and highly volatile flavour ingredients, such as acetoin and diacetyl at high efficiency. More particularly, it involves the production of edible microparticles comprising a matrix of essentially water-insoluble shape-retaining alginate gel held together by salt bridges.
  • the process consists of the following steps:
  • beads are defined as solid particles with a homogeneous composition and texture from inside to outside in which the flavour droplets or particles are uniformly distributed.
  • Capsules are defined as particles consisting of a liquid or solid core of the active ingredient surrounded by a shell.
  • the dry encapsulation process according to the invention overcomes the difficulties encountered in the encapsulation of water-soluble flavours when using the above-described wet slurry technologies of coacervation and absorption into microorganisms.
  • Flavour microparticles produced according to the invention substantially retain their structural integrity in food processes, thus allowing effective protection of the flavour ingredients against volatilization and decomposition. If the active ingredient is a flavour, the flavour microparticles provide sustained release of the flavour to the finished product during storage and prior to consumption. The method accordingly provides a inexpensive method of enhancing flavour effectiveness by preventing flavour loss and/or enhancing flavour release.
  • the production of the flavour microparticles starts with the preparation of an emulsion consisting of a dispersed oil phase in an aqueous solution of an alkali metal alginate.
  • the oil phase may consist of a vegetable oil, a molten fat or any other lipid material that has good flavour solvent properties and is suitable for human ingestion.
  • an emulsifier and an extender or filler material may be added.
  • Non-volatile, poorly water-soluble flavour ingredients may also be added at this stage.
  • the emulsion is dripped or sprayed into an aqueous or alcoholic solution of multivalent cations, which are preferably calcium ions, to convert the droplets into shape retaining, water-insoluble gel microparticles.
  • multivalent cations which are preferably calcium ions
  • the gel particles are isolated from the resulting suspension or slurry of gel beads by filtration or centrifugation.
  • the resulting moist flavour microparticles may be mixed with an anti-caking agent to obtain a free flowing product.
  • this product may be further dried at atmospheric or reduced pressure to obtain a product with a minimum amount of residual water and/or alcohol.
  • the microparticles thus produced are mechanically stable.
  • the dried "blank” gel microparticles are loaded with flavour by mixing the flavour with the microparticles.
  • the flavour is allowed to be absorbed or adsorbed into the microparticles, which might take a few days. This results in a uniform distribution of the flavour over the microparticles.
  • the major part of the equilibration may also take place in a package.
  • the microparticles may be equilibrated at elevated temperature.
  • the process is cost-effective and gives efficient encapsulation of volatile and water-soluble flavours. It allows encapsulation of flavourings of different consistency, water-solubility and volatility. Further, the process allows manipulation of flavour retention and release by use of filler materials, adsorbents or flavour solvents with different melting points.
  • the microparticles may be coloured by the addition of a colouring material to the abovementioned process.
  • the microparticles have a unique combination of desirable properties. They may have different shape varying from beads to fibers and can contain different concentrations of flavour oils and/or solid flavour materials, varying from less than 1 to more than 80% by weight.
  • the microparticles of this invention can much better withstand the harsh conditions during food processing than any other microcapsules currently being used for flavour encapsulation. For example, they are heat- and freeze-stable both in dry and moist environments, and they can withstand high shear conditions. They are thus especially advantageous in food processes in which such conditions occur.
  • an alkali metal alginate preferably sodium alginate
  • water is dissolved in water to produce a solution containing between about 1 and 5% by weight of the alginate. All hereafter mentioned percent values are percent values by weight. Concentrations of alginate below about 0.5% are increasingly ineffective in producing defect-free microcapsules. Alginate concentrations above 4%, although desirable for reasons of encapsulation effectiveness, are often too viscous to allow formation of small beads of uniform size.
  • pectin or gellan gum may also be used in this process.
  • Alginates are linear copolymers of a- L -guluronate (G) and b- D -mannuronate (M).
  • the alginate chain may be regarded as a block copolymer consisting of "G-blocks” (homopolymeric regions of guluronate residues) "M-blocks” (homopolymeric regions of mannuronate residues) and "MG blocks” (copolymeric regions of a random-like alternating sequence of M and G) of varying length.
  • G-blocks homopolymeric regions of guluronate residues
  • M-blocks homopolymeric regions of mannuronate residues
  • MG blocks copolymeric regions of a random-like alternating sequence of M and G
  • the properties of the alginates are mainly governed by the monomeric composition and block structure.
  • an increase in the content of guluronate gives mechanically stronger gels with enhanced stability in the presence of non-gelling/anti-gelling ions (e.g. Na + , Mg 2+ ) and calcium sequestering agents.
  • Gels with a high guluronate content exhibit high porosity and low shrinkage during gel formation.
  • the gels become softer and more elastic; they shrink more during gel formation with concomitant reduction of porosity.
  • all types of alginate can be used but those with a high molecular weight are generally preferred because their high mechanical stability makes them more effective.
  • the structurally-related pectin may be used for the production of water-insoluble, heat-stable gel beads.
  • Pectin is a hydrocolloid consisting of polygalacturonic acid of which the carboxylic acid groups are partly esterified with methanol.
  • Gellan gum is a high-molecular-weight heteropolysaccharide consisting of a linear tetrasaccharide repeat structure comprising 1,3- ⁇ -D-glucose, 1,4- ⁇ -D-glucuronic acid, 1,4- ⁇ -D-glucose and 1,4- ⁇ -L-rhamnose. It forms gels with several counter ions of which the divalent ions, such as calcium and magnesium, give maximum gel hardness. Gels formed in the presence of calcium ion concentrations higher than 10mM are heat stable under normal food processing conditions.
  • the relatively large pore size of the heat-stable polysaccharide gel beads restricts the capability of alginate gels to act as an insurmountable barrier for small molecules, such as flavour molecules, vitamins, etc. Nevertheless, an alginate gel may sustain the release of molecules to a different extent, depending on the barriers within the gel. If, for example, the gel contains other (macro)molecules, the effective porosity will decrease and the sustained release will be at a lower rate. For this reason, it is sometimes advantageous to add a filler material such as native starch or silicon dioxide to the alginate solution.
  • suitable filler materials include polysaccharides such as dextrins, dextran, locust bean gum, gum arabic and methyl cellulose, ethyl cellulose, hydroxypropyl cellulose and proteins, such as gelatine.
  • emulsifiers such as octenyl succinated starch and mono- and diglycerides, or mixtures of mono- and diglycerides, may be added to the aqueous solution of the acid polysaccharide. These emulsifiers help to obtain an oil-in-water emulsion of high stability, which is a prerequisite for the formation of beads of constant composition and size.
  • water-insoluble flavour solvent useful in the practice of the invention are vegetable oils, solid fats of different melting point and mono- or diglycerides.
  • a lipophilic fat replacer for example, a sucrose polyester such as Olestra® (Procter & Gamble), may be used.
  • water-insoluble flavour carriers such as silicon dioxide may be added as well as colouring materials and non-volatile flavour ingredients, such as aspartame or capsaicin.
  • the resulting two phase system is subjected to rapid stirring to induce emulsification of the oil phase in the aqueous phase.
  • a homogenizer or another high shear mixing apparatus is useful for this step.
  • the resulting particle or oil droplet size in the emulsion is in the 1-10 micrometer range to ensure good stability of the suspension or emulsion during at least the period of bead formation (up to a few hours).
  • the gel particles are being prepared using one of the following methods.
  • One of the preferred methods of gel bead production consists of generating droplets by spraying using a nozzle or disk and collecting the droplets, while substantially spherical, in a multivalent cation-containing solution, e.g., an aqueous or alcoholic solution of calcium chloride.
  • the droplets are of a size preferably within the range of about 100-5000 micrometers.
  • the alkali metal counter-ions of the acid polysaccharide are exchanged by calcium ions, resulting in instantaneous gelation of the droplets through the formation of multiple salt bridges between the acid polysaccharide molecules.
  • Another method of droplet generation consists of extruding or pumping the emulsion through a needle or orifice at a speed slow enough to prevent the formation of a jet.
  • This method provides beads of very uniform size but the production capacity is low. Much higher capacity is achieved by making use of a resonance technique which consists of breaking up a jet of the emulsion into uniform droplets by means of a resonanation ( A.C. Hulst, J. Tramper, K. van't Riet and J.M.M. Westerbeek, Biotechnol. Bioeng. 27, 870-876 [1985] ). Therefore, the latter method is preferred for the large-scale industrial production of the gel beads.
  • Still another method for the production of polysaccharide gel microparticles consists of preparing a gel using mixtures consisting of a sodium salt of an acid polysaccharide and one other gel-forming polymer such as agar, and to break the gel into small particles by shear. Subsequently, a concentrated solution of calcium chloride is added to convert the water-soluble salt of the acid polysaccharide into an insoluble calcium salt in order to obtain microparticles of high heat stability.
  • the particles obtained by this method have an irregular shape, which might be an advantage in some applications. In principle, particles of any shape can be used for the flavour encapsulation, provided that the dimensions are not so extreme that the flavour retention and release are adversely affected.
  • Calcium ions in the concentration range of 1-10 % are the preferred multivalent cations for alginate gelation because of their high effectiveness, low costs and low toxicity.
  • other metal ions such as strontium, barium, iron, silver, aluminum, manganese, copper or zinc ions may also be used.
  • strontium, barium, iron, silver, aluminum, manganese, copper or zinc ions may also be used.
  • a skin of insoluble calcium alginate forms at once on the outside. Thereafter, calcium ions diffuse slowly into the drops and so a reasonable time is necessary for full conversion to solid gelled particles.
  • the contact time should be from 1 to 500 minutes.
  • low molecular mass alginate low concentration of gelling ions and absence of non-gelling ions give the highest inhomogeneity, whereas a high molecular weight polysaccharide, and a high concentration of non-gelling ions all give increased homogeneity.
  • the preferred solvents for the solution of multivalent cations are water and/or a low molecular weight alcohol such as methanol, ethanol and isopropyl alcohol. Higher molecular weight alcohols may also be used, but the low molecular weight alcohols are preferred because they can be removed more easily from the micro-beads by volatilzation.
  • water is the preferred solvent.
  • alcohol is the preferred solvent because it precipitates the water-soluble filler within the gel matrix.
  • microparticles prepared by one of the above methods can be isolated from the slurry by filtration or centrifugation. Optionally, they are washed with water, alcohol or a mixture of water and alcohol to remove adhering sodium and calcium salts.
  • starch, silicon dioxide (e.g. Syloid®), maltodextrin or any other water binding material can be added after isolation. Since different combinations of flavour (solvent) and acid polysaccharide cause different shrinkage during drying, the volume of flavour oil in the original emulsion should be optimized for different polysaccharide in order to obtain dry particles with little surface oil and a minimum tendency to stick together.
  • the water-insoluble gel particles consisting of a porous gel network containing entrapped flavour solvent, are loaded with flavour by mixing the liquid flavour with the particles while tumbling over in a blender or dryer. If the particles contain solid fat, it might be advantageous to use slightly elevated temperature to enhance the rate of flavour diffusion into the particles. When most of the flavour has been absorbed by the particles and the particles do no longer have a strong tendency to stick together, they are transferred into bottles or drums where they are allowed to equilibrate for a few days to achieve uniform distribution of the flavour over the beads by migration. If the beads remain sticky, additional starch or other anti-caking agent is added to obtaining a free flowing product.
  • flavours and flavour ingredients may be encapsulated in the gel microparticles.
  • These flavours include flavour compounds, and complex mixtures such as extracts, essential oils, oleoresins or reconstituted natural, nature-identical or artificial flavours.
  • Natural extracts, essential oils and oleoresins include fruit essences, vanilla extract, capsicum oleoresin, pepper oleoresin, cinnamon oil, oil of winter green, peppermint oil, bay oil, thyme oil, spearmint oil, cassia oil, citrus oils, and the like.
  • Reconstituted natural, nature-identical and artificial flavours include apple, cherry, strawberry, peach as well as meat, cheese, tomato and butter flavours. These flavourings may be used individually or in a mixture as is well known in the art.
  • the heat-stable, sustained-release polysaccharide gel beads as obtained by the processes according to the invention may be employed to improve flavour impact in a wide variety of food applications.
  • encapsulation in a multivalent cation-containing acid polysaccharide matrix may be used to protect the flavour against volatilization and chemical decomposition during heat processing.
  • the term "heat-stable” as used herein means protected against deteriorating effects of heat under dry and/or moist conditions.
  • the heat-stable polysaccharide microparticles are particularly suited for improving flavour retention in solid or semi-solid foods during microwave heating, boiling, cooking, baking, frying, roasting, drying, and extrusion. Moreover, they are able to protect flavours in liquid products such as soups and sauces against chemical decomposition or volatilization during retorting, boiling, pasteurization or sterilization.
  • Dried gel microparticles are preferred for use in products that require heat processing to produce the finished product.
  • the performance of dry microparticles is much superior to the performance of wet microparticles such as slurries and filtered beads (moisture content more than 50%), and slightly superior to microparticles isolated by centrifugation (moisture content of stach coated beads 15-20%).
  • Study of the relationship between flavour loss during heat processing and the steam volatility of the flavour constituents strongly suggests that steam distillation from the microenvironment of the moist flavour beads is the major cause of the flavour losses from moist gel particles. Since dry calcium alginate does not easily rehydrate, a low moisture microenvironment is maintained around the flavour during the initial period of the heat processing thus resulting in the superior performance of the dry alginate beads as compared to the wet beads.
  • Sodium alginate (type Protanal LF 20/60 ex Pronova or FD 155, Grinsted; 8.22 g) was dissolved in demineralized water (300g) with stirring to produce a homogeneous aqueous solution.
  • Capsul (4.5 grams) was added and stirri ng was continued till a homogeneous phase was obtained.
  • miglyol (99.9 grams) was added to the solution and the two-phase mixture was emulsified by vigorous stirring with an Ultra-Turrax apperatus to form a stable oil-in-water emulsion.
  • the emulsion was fed through a vibrating needle of 1.22 mm internal diameter disposed about one inch above the lowest point of an eddy that was generated in a glass beaker by vigorous stirring 441 mL of a 1.6% solution of calcium chloride dihydrate in water.
  • the flow rate through the needle was adjusted to prevent the formation of a jet.
  • the emulsion droplets upon entering the calcium chloride solution, immediately gelled to yield particles of about 800 micrometer diameter.
  • the slurry of beads was allowed to stand for 16 hours to ensure complete penetration of the calcium ions into the beads.
  • the beads were isolated by filtration. Prior to filtration, the slurry of beads was sometimes sieved in order to obtain a fraction of uniform particle size (710-1000 mm) for comparative performance tests.
  • the filtered beads (moisture content 50-55%) were dried in an oven at reduced pressure at room temperature to yield a dry product.
  • the particle size of the dry beads produced by this method is in the range of 500-1000 mm.
  • the particle size of the wet beads in aqueous slurry was measured by Coulter Counter LS 200 particle size analyzer.
  • the particle size given in the Examples is the modal value for the wet beads in aqueous slurry, unless specified otherwise.
  • the particle size of the dry beads was measured in suspension in propylene glycol.
  • the alginate gel beads were loaded with flavour by dripping the liquid flavour oil on the beads while stirring. Depending on the type of flavour, the process was carried out at room temperature if the flavour solvent was a liquid oil or at elevated temperatures if the solvent was solid fat. The beads were then allowed to stand for 1 hour till 5 days to allow complete absorption of the flavour oil. Depending on the flavour solvent in the beads and the flavour load, a more or less free flowing product was obtained in which the particles have sometimes a slight tendency to stick together due to the presence of some surface oil.
  • Sodium alginate (type Protanal LF 20/60 ex Pronova; 4.11 kg) was dissolved in tap water (150 kg) in a 500 L tank to produce a homogeneous aqueous solution. The solution was circulated to speed up the dissolution of the alginate. Capsul (2.25 kg) was added and stirring was continued till a homogeneous phase is obtained. Subsequently, miglyol (50 kg) was added to the solution and the two-phase mixture was emulsified in portions by vigorous stirring with an Ultra-Turrax. The emulsion, maintained at a temperature of 40°C, was sprayed on a Pilot BioSphere Sprayer (Landteknikk, Oslo, Norway).
  • the disk which is equipped with a rotating disk that contains specially designed holes for ejecting the emulsion in droplets of uniform size.
  • the disk holes are 0.8 mm, the feed flow 1 kg/min and the disk speed 374 rpm.
  • the size of the droplets depends on the viscosity of the emulsion and the speed of the rotation.
  • the droplets were collected in 1200 kg of a solution of 1.6 % calcium chloride dihydrate in water.
  • the beads were isolated by filtration. Prior to filtration, part of the slurry of beads was sieved in order to obtain a fraction of uniform particle size (diameter between 710 mm and 1000 mm) for comparative performance tests.
  • the filtered gel beads were dried in a (vacuum) oven at 20 °C and loaded with flavour as described in Example 1. If the beads remained a little bit sticky after loading with flavour, additional starch was added to obtain a free flowing product.
  • Example 2 This example is equivalent to Example 1 except for the coating with starch. Coating was carried out after filtration. The filtered gel beads moisture content 50-55%) were coated by mixing with corn starch (30 g per 100 g of wet beads). The resulting mixture was stirred or shaken till a free flowing product was obtained. Optionally, the beads were dried in a (vacuum) oven and loaded with flavour as described in Example 1. If the beads remained a little bit sticky after loading with flavour, additional starch was added to obtain a free flowing product.
  • This example is equivalent to Example 2 except for the isolation and drying of the gel beads.
  • the gel beads were isolated by centrifugation (moisture content about 20%) and either:
  • the beads were loaded with flavour as described in example 1. If the beads remained a little bit sticky after loading with flavour, additional starch was added to obtain a free flowing product.
  • Example 2 This example is equivalent to Example 1, except for the flavour solvent which was refined soy oil instead of miglyol.
  • This example is equivalent to Example 1, except for the following differences: hydrogenated palm kernel oil instead of miglyol was used as the flavour solvent and silicon dioxide (Hubersil 1714, ex J.M. Huber Corporation) was added as an adsorbent The temperature of the emulsion was maintained at 50°C to keep the palm oil in melted form.
  • hydrogenated palm kernel oil instead of miglyol was used as the flavour solvent and silicon dioxide (Hubersil 1714, ex J.M. Huber Corporation) was added as an adsorbent
  • the temperature of the emulsion was maintained at 50°C to keep the palm oil in melted form.
  • This example is equivalent to Example 3, except for the incorporation of gelatin in the gel matrix.
  • the amount of gelatin used (Gelatine 280/300 Bloom ex Bovines) was 1 g/ g of sodium alginate.
  • the resulting slurry of beads was sieved to collect a fraction with a particle size of 710 - 1000 mm. Subsequently, the beads were:
  • the cross-linking was carried our by adding 76 g of filtered beads to 78 g of an aqueous 0.086% (w/w) solution of glutaraldehyde. The slurry was stirred overnight, and the beads were collected by filtration, coated with corn starch and dried in a vacuum oven at 1 mm Hg at a constant temperature of 20 °C. Finally, the beads were loaded with flavour as described in Example 1.
  • This example is equivalent to Example 3, except for the use of pectin (type LM 1912 CSZ, Copenhagen Pectin) instead of sodium alginate.
  • the pectin concentration in water is 3% compared to an sodium alginate concentration of 2%.
  • the pectin was dissolved at 60°C and then allowed to cool down to room temperature before starting droplet generation.
  • This example is equivalent to Example 1, except for the use of gellan gum (Kelcogel F, Kelco) instead of sodium alginate.
  • the gellan gum concentration in water was 1.5% compared to an sodium alginate concentration of 2%.
  • the gellan gum was dissolved at 50°C and maintained at that temperature during droplet generation.
  • This example shows the effect of the moisture content of the alginate gel beads on the flavour retention in crackers during baking.
  • the alginate beads were prepared according to Example 4 using sodium alginate type LF 20/60 L (Pronova).
  • the flavour load (neat apple flavour without solvent) was 20%, calculated on dry weight basis, i.e. 1 part of flavour to 4 parts of dry uncoated beads.
  • the crackers were prepared according to the following recipe: Ingredient Weight percent Group Biscuit flour 53.80 A Modified starch (C*top) 3.00 A Tetra sodium pyrophosphate 0.10 A Sodium bicarbonate 0.20 A Dextrose 2.50 A Skimmed milk powder 4.00 A Salt 1.50 A Monosodium glutamate 0.40 A Lecithin M30 0.40 A Ammonium bicarbonate 2.00 C Biskien soft (fat) 9.00 B Sodium metabisulfite (10% in water) 0.10 D Water 23.00 C Flavour: Variable* B Total: 100.00 * The dosage of unencapsulated flavour (neat flavour without solvent!) was 3.2 g/kg of dough or an equivalent amount of encapsulated flavour.
  • the results of the organoleptic analysis are in agreement with those of the chemical analysis which shows an increase of flavour retention with a decrease of the moisture content of the beads.
  • the flavour retention was determined as the difference between the flavour concentrations in dough and cracker taking into account the loss of water during baking.
  • This example shows the effect of encapsulation on flavour retention during extrusion.
  • Dry beads were prepared according to the method of Example 1, using alginate type FD 155 (Grindsted). The beads were loaded with apple flavour (2g flavour per 8g of dried beads). The performance of the encapsulated flavour in extruded cereals was compared with that of the unencapsulated liquid flavour oil.
  • the corn curls were prepared according to the following recipe: Ingredient Weight Corn grit 2790 g Water 210.0 g Salt 30.0 g Mono sodium glutamate 12.0 g Flavor Variable* Total 3042.0 g * The dosage of unencapsulated flavour (neat flavour without solvent!) was 2.5 g/kg of grit or an equivalent amount of encapsulated flavour.
  • the flavour was mixed into the corn grit.
  • the salt and monosodium glutamate were dissolved in the water and the resulting solution is added to the flavoured corn grit.
  • the mixture was extruded on a counter-rotating twin screw extruder (exit temperature: 85°C), cut in small pieces and air dried.
  • the corn curls were evaluated on smell (aroma perception by sniff) and taste (aroma perception by mouth).
  • the intensity of the smell is an indication for the amount of the flavour that has been released from the flavour beads into the product prior to consumption.
  • the taste intensity is a measure for the total amount of flavour that was released from the product base and the flavour beads.
  • the results of the organoleptic evaluation are shown below: Particle Intensity of aroma** by Size ( ⁇ m) Sniff Mouth Unencapsulated flavour 2.80 5.20 Encapsulated flavour 1035 3.60 7.00 ** see Example 10
  • the alginate beads were prepared by spraying using a method similar to that of Example 2.
  • the slurry of beads was fractionated by sieving to yield fractions of the following particle size: 0-250, 250-500, 500-1000 and 1000-2000 mm.
  • the dry beads were loaded with apple flavour to yield flavoured beads containing 20% of flavour.
  • the performance of the encapsulated flavours was evaluated in crackers which were prepared as described in Example 10.
  • a cheese top note flavour Gouda type, was encapsulated in dry alginate beads prepared by the method of Example 1 at a load of 20% (w/w).
  • the encapsulated flavour was evaluated in crackers against the unencapsulated flavour as described in example 10. The results show that encapsulation results in a superior flavour performance: Particle Intensity of aroma** by Size ( ⁇ m) Sniff Mouth Unencapsulated flavour 4.33 4.33 Alginate beads 830 7.67 7.42 ** see Example 10
  • alginate encapsulated apple flavour was evaluated in pasta; different flavour solvents were used, miglyol and reveal BEP which is a fractionated, hydrogenated, refined vegetable fat of non-lauric origin, slip melting point 43.0°C (Loders Crocklaan).
  • the pasta was prepared according to the following recipe: Ingredients % by weight Grams per 500 g batch Flour (Semolina) 68.15 340.75 Salt 2.87 14.35 Water 28.98 144.90 Total: 100.00 500.00
  • flavour stability during storage is highest if the flavours are encapsulated.
  • the differences are most pronounced during consumption (flavour perception by mouth). This suggests that the flavour is effectively encapsulated and that the encapsulation has a positive effect on the flavour release during consumption.
  • Chemical analysis confirmed this conclusion.
  • the differences in flavour concentration between the pastas are smaller than expected on the basis of the organoleptic evaluations. This suggests that part of the difference in flavour strength has to be attributed to improvement of flavour release.
  • Dry alginate beads are loaded with a mustard flavour (20% load) that contains allyl isothiocyanate as the active principle using the method of example 1.
  • the loaded flavour beads are evaluated in chicken nuggets using the following recipe: Ingredients of adhesion batter Weight % Water 67.00 Batter mix N0004 NFI * 33.00 Total 100.00 * Contains wheat flour, hydrocolloids, white of egg and salt.

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EP03018435A 1996-10-09 1997-10-08 Use of beads as food additives Expired - Lifetime EP1369043B1 (en)

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EP0936877A1 (en) 1999-08-25
HUP9904115A3 (en) 2001-01-29
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EP1369043A1 (en) 2003-12-10
CA2267116A1 (en) 1998-04-16
HUP9904115A2 (hu) 2000-04-28
WO1998015192A1 (en) 1998-04-16
JP2001507926A (ja) 2001-06-19
AU733927B2 (en) 2001-05-31
US20030082272A1 (en) 2003-05-01
US6436461B1 (en) 2002-08-20
PL332669A1 (en) 1999-09-27
DE69726446T2 (de) 2004-08-26
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US6929814B2 (en) 2005-08-16
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